Use of a nanoindentation fatigue test to characterize the ductile–brittle transition

When considering grinding of minerals, scaling effect induces competition between plastic deformation and fracture in brittle solids. The competition can be sketched by a critical size of the material, which characterizes the ductile–brittle transition. A first approach using Vickers indentation gives a good approximation of the critical size through an extrapolation from the macroscopic to the microscopic scales. Nanoindentation tests confirm this experimental value. According to the grain size compared to the indent size, it can reasonably be said that the mode of damage is deformation-induced intragranular microfracture. This technique also enables to perform cyclic indentations to examine calcite fatigue resistance. Repeated loadings with a nanoindenter on CaCO3 polycrystalline samples produce cumulative mechanical damage. It is also shown that the transition between ductile and brittle behaviour depends on the number of indentation cycles. The ductile domain can be reduced when the material is exposed to a fatigue process.